CN116695446B - Fabric with infrared shielding function and preparation method thereof - Google Patents

Fabric with infrared shielding function and preparation method thereof Download PDF

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CN116695446B
CN116695446B CN202310849188.6A CN202310849188A CN116695446B CN 116695446 B CN116695446 B CN 116695446B CN 202310849188 A CN202310849188 A CN 202310849188A CN 116695446 B CN116695446 B CN 116695446B
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infrared shielding
fabric
mass
stirring
allyl
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CN116695446A (en
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赵栋炜
肖子良
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Wujiang Xingye Textile Co ltd
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Wujiang Xingye Textile Co ltd
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55—Epoxy resins
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325—Amines
    • D06M13/332—Di- or polyamines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/657—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing fluorine
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a fabric with an infrared shielding function and a preparation method thereof, and relates to the technical field of textile materials. When the fabric with the infrared shielding function is prepared, firstly, chromium-doped nano cesium tungsten bronze, allyl trimethoxysilane and dimethyl dimethoxy silane are reacted, and then the modified chromium-doped nano cesium tungsten bronze is prepared by reacting with 3-glycidol ether oxypropyl dimethoxy silane; preparing hydrogen-containing silicone oil, 1, 7-divinyl-octamethyltetrasiloxane and N-allyl heptafluorobutyramide into mixed silicon liquid; uniformly mixing epoxy resin, modified chromium doped nano cesium tungsten bronze, mixed silicon liquid, poly N-aminoethyl-3-aminopropyl methyl siloxane and xylene to prepare infrared shielding treatment liquid; and (3) sequentially treating the polyester fibers by using ethylenediamine and infrared shielding treatment liquid, and weaving the polyester fibers into the fabric with an infrared shielding function. The fabric with the infrared shielding function prepared by the invention has excellent infrared shielding performance, fracture resistance and acid and alkali resistance.

Description

Fabric with infrared shielding function and preparation method thereof
Technical Field
The invention relates to the technical field of textile materials, in particular to a fabric with an infrared shielding function and a preparation method thereof.
Background
With regard to stealth means, it has long been used by people, for example, original humans draw a bright colored pattern on their bodies during hunting to hide their own actions, thereby better approaching the hunting and capturing the hunting. In ancient and modern wars, people can disguise themselves by using natural environments where the people are located, for example, in jungle wars, fighters can disguise themselves by using green plants, leaves or withered grass, so that the people are prevented from being found by enemies, and attack can be initiated inadvertently, and the enemies can be given the greatest degree of attack. Modern camouflage is developed from the second battle, the current soviet battle field is frequently hit by the German air force, many important military facilities are destroyed, and the loss of personnel is also large. In this context, the scientist involved invents a simple trichromatic camouflage fabric for camouflage of military facilities, and this simple application greatly reduces the probability of the German air force to find ground military facilities, thus reducing the losses of the wars in war and retaining the productive forces for the counterattack after the soviet union.
However, with the wide application of modern advanced detection technology and accurate guided weapon in battlefield, the conventional visible camouflage technology cannot meet the requirements of the current battlefield. At present, with the application of detection means such as night vision goggles, thermal infrared imaging, radars, lasers, advanced satellite systems and the like in military, the situation of a battlefield becomes worse, and in order to master the initiative of the battlefield, more and more countries have increased investment in infrared stealth. Therefore, the infrared shielding functional fabric has great research and development value.
Disclosure of Invention
The invention aims to provide a fabric with an infrared shielding function and a preparation method thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the fabric with the infrared shielding function is characterized in that the fabric with the infrared shielding function is prepared by uniformly mixing epoxy resin, modified chromium doped nano cesium tungsten bronze, mixed silicon liquid, poly N-aminoethyl-3-aminopropyl methyl siloxane and xylene to prepare an infrared shielding treatment liquid; and (3) carrying out aminolysis on the polyester fiber by using ethylenediamine, immersing the polyester fiber in the infrared shielding treatment liquid, taking out, heating, standing and drying to obtain the infrared shielding fiber, and weaving the infrared shielding fiber.
As optimization, the modified chromium-doped nano cesium tungsten bronze is prepared by carrying out solvothermal reaction on tungsten chloride, chromium trichloride hexahydrate and cesium hydroxide monohydrate to obtain the chromium-doped nano cesium tungsten bronze, and then carrying out reaction on the chromium-doped nano cesium tungsten bronze, allyl trimethoxysilane and dimethyl dimethoxy silane and then carrying out reaction on the chromium-doped nano cesium tungsten bronze and 3-glycidol ether oxypropyl dimethoxy silane.
As optimization, the mixed silicon liquid is prepared by uniformly mixing hydrogen-containing silicone oil, 1, 7-divinyl-octamethyltetrasiloxane and N-allyl heptafluorobutyramide.
Preferably, the N-allyl heptafluorobutylamine is prepared by reacting heptafluorobutyric acid with thionyl chloride and then reacting with allylamine.
As optimization, the preparation method of the fabric with the infrared shielding function comprises the following preparation steps:
(1) Uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.1-0.2% according to the mass ratio of 4-6:3-4:2:1, stirring and refluxing for 20-30 min at 65-70 ℃ and 200-300 r/min, adding chromium doped nano cesium tungsten bronze with the mass of 0.8-1 times of the allyl trimethoxysilane, continuously stirring and refluxing for 60-80 min, adding 3-glycidoxypropyl dimethoxy silane with the mass of 0.2-0.3 times of the allyl trimethoxysilane and a hydrochloric acid aqueous solution with the mass fraction of 0.1-0.2% with the mass fraction of 0.04-0.06 times of the allyl trimethoxysilane, continuously stirring and refluxing for 40-50 min, centrifugally separating and washing 3-5 times with absolute ethyl alcohol to obtain modified chromium doped nano cesium tungsten bronze;
(2) Weighing according to the molar ratio of silicon-hydrogen bond in hydrogen-containing silicone oil to vinyl in 1, 7-divinyl-octamethyltetrasiloxane to allyl in N-allyl heptafluorobutyramide of 1:0.4-0.6:0.1-0.2, uniformly mixing the hydrogen-containing silicone oil, the 1, 7-divinyl-octamethyltetrasiloxane and the N-allyl heptafluorobutyramide, and adding chloroplatinic acid with the mass of 0.003-0.005 times that of the hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing epoxy resin, modified chromium-doped nano cesium tungsten bronze, mixed silicon liquid and dimethylbenzene according to a mass ratio of 6-8:3-3.5:4-5:1, stirring for 20-25 min at 20-30 ℃ at 200-300 r/min, adding poly-N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.25-0.3 times of that of the epoxy resin, and continuously stirring for 8-10 min to prepare an infrared shielding treatment liquid;
(4) Immersing polyester fiber in 0.8-1% of ethylene glycolStanding for 20-30 min at 50-70 ℃ in an amine aqueous solution, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying for 4-6 h at 60-70 ℃ to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 6-8 min at 20-30 ℃ and 25-35 kHz, taking out until 30-40 s have no dripping, sequentially standing for 4-5 min at 110-120 ℃, standing for 1-2 h at 60-70 ℃, and standing for 10-12 h at 40-50 ℃ and 50-100 Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into the fiber with the gram weight of 200 to 300g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
As optimization, the preparation method of the chromium-doped nano cesium tungsten bronze in the step (1) comprises the following steps: uniformly mixing tungsten chloride and absolute ethyl alcohol according to the mass ratio of 1:120-140, adding hexahydrated chromium trichloride with the molar quantity of tungsten chloride of 0.14-0.16 times, stirring at 20-30 ℃ for reaction for 30-40 min at 200-300 r/min, adding cesium hydroxide monohydrate with the molar quantity of tungsten chloride of 0.3-0.34 times, continuously stirring for 20-30 min, adding absolute acetic acid with the mass of 30-40 times of tungsten chloride, continuously stirring for 10-15 min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 210-220 ℃ for 20-24 h, cooling to room temperature, centrifuging, separating at 10-15 ℃ and drying at 10-50 Pa for 6-8 h to prepare the catalyst.
As optimization, the preparation method of the N-allyl heptafluorobutyramide in the step (2) comprises the following steps: uniformly mixing heptafluorobutyric acid, thionyl chloride and tetrahydrofuran according to the mass ratio of 1:5-6:0.03-0.04, stirring at the temperature of 40-50 ℃ for reaction for 50-60 min at the speed of 300-500 r/min, heating to the temperature of 60-70 ℃, stirring and refluxing for 2-3 h, and drying at the temperature of 90-100 ℃ for 4-6 h to obtain heptafluorobutyryl chloride; uniformly mixing heptafluorobutyryl chloride and allylamine according to a molar ratio of 1:2-3, adding triethylamine with the mass of 0.3-0.4 times that of the heptafluorobutyryl chloride, stirring for 2-3 hours at the temperature of 0-5 ℃ and the speed of 300-500 r/min, and drying for 4-6 hours at the temperature of 90-100 ℃ to prepare the compound aqueous emulsion.
Preferably, the hydrogen-containing silicone oil in the step (2) is 202 methyl hydrogen-containing silicone oil.
As an optimization, the epoxy resin in the step (3) is bisphenol a type epoxy resin; the dimethylbenzene is one or more of paraxylene, metaxylene and orthoxylene.
As optimization, the polyester fiber in the step (4) is 75D/36F polyester fiber.
Compared with the prior art, the invention has the following beneficial effects:
when the fabric with the infrared shielding function is prepared, epoxy resin, modified chromium doped nano cesium tungsten bronze, mixed silicon liquid, poly-N-aminoethyl-3-aminopropyl methyl siloxane and dimethylbenzene are uniformly mixed to prepare infrared shielding treatment liquid; and (3) carrying out aminolysis on polyester fibers by using ethylenediamine, immersing the polyester fibers in infrared shielding treatment liquid, taking out, heating, standing and drying to obtain infrared shielding fibers, and weaving the infrared shielding fibers into the fabric with an infrared shielding function.
Firstly, carrying out solvothermal reaction on tungsten chloride, chromium trichloride hexahydrate and cesium hydroxide monohydrate to obtain chromium-doped nano cesium tungsten bronze, wherein the chromium and tungsten belong to the same subgroup, and the ion radius is close, so that the doped nano cesium tungsten bronze can partially replace tungsten, and the crystal defect is further increased, thereby improving the infrared shielding performance; the chromium-doped nano cesium tungsten bronze is modified, and a polysiloxane long chain is formed on the surface of the modified chromium-doped nano cesium tungsten bronze, so that the compatibility of the chromium-doped nano cesium tungsten bronze with other components is improved, the chromium-doped nano cesium tungsten bronze is not easy to agglomerate, meanwhile, the polysiloxane long chain contains a large number of carbon-carbon double bonds and epoxy groups, the carbon-carbon double bonds can react with silicon hydrogen bonds on hydrogen-containing silicone oil in a silicon-hydrogen addition manner, and the epoxy groups can react with amino groups, so that a cross-linked network structure is formed, the structure is more compact and stable, and the fracture resistance and acid-alkali resistance are improved.
Secondly, reacting heptafluorobutyric acid with thionyl chloride, and then reacting with allylamine to prepare N-allylheptafluorobutylamine; the method comprises the steps of uniformly mixing hydrogen-containing silicone oil, 1, 7-divinyl-octamethyltetrasiloxane and N-allyl heptafluorobutyramide to prepare mixed silicon liquid, wherein the mixed silicon liquid can be subjected to hydrosilylation reaction, and is crosslinked and cured with epoxy resin to form an interpenetrating network structure, and the N-allyl heptafluorobutyramide introduces heptafluorobutyramide branched chains on the hydrogen-containing silicone oil, so that the main chain has good protection effect, the corrosion of corrosive medium is effectively relieved, and the acid-base resistance is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The method provided by the present invention is described in detail by the following examples for more clarity of illustration.
Example 1
The preparation method of the fabric with the infrared shielding function mainly comprises the following preparation steps:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to a mass ratio of 1:120, adding chromium trichloride hexahydrate with a molar quantity of 0.14-0.16 times of the tungsten chloride, stirring at 20 ℃ for reaction for 30min at 200r/min, adding cesium hydroxide monohydrate with a molar quantity of 0.3 times of the tungsten chloride, continuously stirring for 20min, adding absolute acetic acid with a mass of 30 times of the tungsten chloride, continuously stirring for 10min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 210 ℃ for 20h, cooling to room temperature, centrifuging, separating, and drying at 10Pa for 8h at 10 ℃ to obtain chromium-doped nano cesium tungsten bronze; uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.1% according to the mass ratio of 4:3:2:1, stirring and refluxing for 20min at 65 ℃ and 200r/min, adding chromium doped nano cesium tungsten bronze with the mass of 0.8 times of the allyl trimethoxysilane, continuously stirring and refluxing for 60min, adding 3-glycidoxypropyl dimethoxy silane with the mass of 0.2 times of the allyl trimethoxysilane and a hydrochloric acid aqueous solution with the mass fraction of 0.1% with the mass fraction of 0.04 times of the allyl trimethoxysilane, continuously stirring and refluxing for 40min, centrifugally separating and washing for 3 times by using absolute ethyl alcohol to obtain modified chromium doped nano cesium tungsten bronze;
(2) Uniformly mixing heptafluorobutyric acid, thionyl chloride and tetrahydrofuran according to a mass ratio of 1:5:0.03, stirring and reacting for 50min at 40 ℃ and 300r/min, heating to 60 ℃, stirring and refluxing for 2h, and drying at 90 ℃ for 6h to obtain heptafluorobutyryl chloride; uniformly mixing heptafluorobutyryl chloride and allylamine according to a molar ratio of 1:2, adding triethylamine with the mass of 0.3 times that of the heptafluorobutyryl chloride, stirring at 0 ℃ and 300r/min for 2h, and drying at 90 ℃ for 6h to obtain N-allyl heptafluorobutyramide; weighing according to the molar ratio of silicon-hydrogen bond in 202 methyl hydrogen-containing silicone oil, the molar ratio of the middle vinyl of 1, 7-divinyl-octamethyl tetrasiloxane and the allyl in N-allyl heptafluoro-butyramide of 1:0.4:0.1, uniformly mixing 202 methyl hydrogen-containing silicone oil, 1, 7-divinyl-octamethyl tetrasiloxane and N-allyl heptafluoro-butyramide, and adding chloroplatinic acid with the mass of 0.003 times that of 202 methyl hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing bisphenol A epoxy resin, modified chromium doped nano cesium tungsten bronze, mixed silicon liquid and paraxylene according to a mass ratio of 6:3:4:1, stirring at 20 ℃ for 20min at 200r/min, adding poly N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.25 times that of the bisphenol A epoxy resin, and continuing stirring for 8min to prepare infrared shielding treatment liquid;
(4) Immersing 75D/36F polyester fibers in an ethylenediamine water solution with the mass fraction of 0.8%, standing for 20min at 50 ℃, taking out, washing with absolute ethyl alcohol for 3 times, and drying at 60 ℃ for 6h to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 6min at 20 ℃ and 25kHz, taking out until no drop exists for 30s, sequentially standing for 5min at 110 ℃, standing for 2h at 60 ℃ and standing for 10h at 40 ℃ and 50Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into a fiber with gram weight of 200g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
Example 2
The preparation method of the fabric with the infrared shielding function mainly comprises the following preparation steps:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to a mass ratio of 1:130, adding chromium trichloride hexahydrate with a molar quantity of 0.15 times of the tungsten chloride, stirring at 25 ℃ for reaction for 35min at 250r/min, adding cesium hydroxide monohydrate with a molar quantity of 0.32 times of the tungsten chloride, continuously stirring for 25min, adding absolute acetic acid with a mass of 35 times of the tungsten chloride, continuously stirring for 17min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 215 ℃ for 22h, cooling to room temperature, centrifuging, separating, and drying at 12.5 ℃ for 7h at 30Pa to obtain chromium-doped nano cesium tungsten bronze; uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.15% according to the mass ratio of 5:3.5:2:1, stirring and refluxing at 67.5 ℃ for 25min at 250r/min, adding chromium-doped nano cesium tungsten bronze with the mass of 0.8-1 times of the allyl trimethoxysilane, continuously stirring and refluxing for 70min, adding a hydrochloric acid aqueous solution with the mass fraction of 0.15% and the mass fraction of 0.25 times of the 3-glycidoxy propyl dimethoxy silane and the allyl trimethoxysilane, continuously stirring and refluxing for 45min, centrifugally separating and washing for 4 times by using absolute ethyl alcohol to obtain modified chromium-doped nano cesium tungsten bronze;
(2) Uniformly mixing heptafluorobutyric acid, thionyl chloride and tetrahydrofuran according to the mass ratio of 1:5.5:0.035, stirring and reacting for 55min at 45 ℃ and 400r/min, heating to 65 ℃ and stirring and refluxing for 2.5h, and drying for 5h at 95 ℃ to obtain heptafluorobutyryl chloride; uniformly mixing heptafluorobutyryl chloride and allylamine according to a molar ratio of 1:2.5, adding triethylamine with the mass of 0.35 times that of the heptafluorobutyryl chloride, stirring at 2.5 ℃ and 400r/min for 2.5 hours, and drying at 95 ℃ for 5 hours to obtain N-allyl heptafluorobutyramide; weighing according to the molar ratio of silicon-hydrogen bond in 202 methyl hydrogen-containing silicone oil, the molar ratio of the middle vinyl of 1, 7-divinyl-octamethyl tetrasiloxane and the allyl in N-allyl heptafluoro-butyramide of 1:0.5:0.15, uniformly mixing 202 methyl hydrogen-containing silicone oil, 1, 7-divinyl-octamethyl tetrasiloxane and N-allyl heptafluoro-butyramide, and adding chloroplatinic acid with the mass of 0.004 times that of 202 methyl hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing bisphenol A epoxy resin, modified chromium doped nano cesium tungsten bronze, mixed silicon liquid and paraxylene according to the mass ratio of 7:3.3:4.5:1, stirring at 25 ℃ for 22.5min at 250r/min, adding poly N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.27 times that of bisphenol A epoxy resin, and continuously stirring for 9min to prepare infrared shielding treatment liquid;
(4) Immersing 75D/36F polyester fibers in an ethylenediamine water solution with the mass fraction of 0.9%, standing at 60 ℃ for 25min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 5h to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 7min at 25 ℃ and 30kHz, taking out until 35s are free from dripping, sequentially standing for 4.5min at 115 ℃, standing for 1.5h at 65 ℃ and standing for 11h at 45 ℃ and 75Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into a fiber with gram weight of 200g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
Example 3
The preparation method of the fabric with the infrared shielding function mainly comprises the following preparation steps:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to a mass ratio of 1:140, adding chromium trichloride hexahydrate with a molar quantity of 0.16 times of the tungsten chloride, stirring at 30 ℃ for reaction for 40min at 300r/min, adding cesium hydroxide monohydrate with a molar quantity of 0.34 times of the tungsten chloride, continuously stirring for 30min, adding absolute acetic acid with a mass of 40 times of the tungsten chloride, continuously stirring for 15min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 220 ℃ for 24h, cooling to room temperature, centrifuging, and drying at 15 ℃ for 6h at 50Pa to obtain chromium-doped nano cesium tungsten bronze; uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.2% according to the mass ratio of 6:4:2:1, stirring and refluxing at 70 ℃ for 30min at 300r/min, adding chromium doped nano cesium tungsten bronze with the mass 1 times of the allyl trimethoxysilane, continuously stirring and refluxing for 80min, adding 3-glycidoxypropyl dimethoxy silane with the mass 0.3 times of the allyl trimethoxysilane and a hydrochloric acid aqueous solution with the mass fraction of 0.2% with the mass 0.06 times of the allyl trimethoxysilane, continuously stirring and refluxing for 50min, centrifugally separating and washing with absolute ethyl alcohol for 5 times to obtain modified chromium doped nano cesium tungsten bronze;
(2) Uniformly mixing heptafluorobutyric acid, thionyl chloride and tetrahydrofuran according to a mass ratio of 1:6:0.04, stirring and reacting for 60min at 50 ℃ and 500r/min, heating to 70 ℃, stirring and refluxing for 3h, and drying for 4h at 100 ℃ to obtain heptafluorobutyryl chloride; uniformly mixing heptafluorobutyryl chloride and allylamine according to a molar ratio of 1:3, adding triethylamine with the mass of 0.4 times that of the heptafluorobutyryl chloride, stirring for 3 hours at 5 ℃ and 500r/min, and drying for 4 hours at 100 ℃ to obtain N-allyl heptafluorobutyramide; weighing according to the molar ratio of silicon-hydrogen bond in 202 methyl hydrogen-containing silicone oil, the molar ratio of the middle vinyl of 1, 7-divinyl-octamethyl tetrasiloxane and the allyl in N-allyl heptafluoro-butyramide of 1:0.6:0.2, uniformly mixing 202 methyl hydrogen-containing silicone oil, 1, 7-divinyl-octamethyl tetrasiloxane and N-allyl heptafluoro-butyramide, and adding chloroplatinic acid with the mass of 0.005 times that of 202 methyl hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing bisphenol A epoxy resin, modified chromium doped nano cesium tungsten bronze, mixed silicon liquid and paraxylene according to a mass ratio of 8:3.5:5:1, stirring at 30 ℃ for 25min at 300r/min, adding poly N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.3 times that of the bisphenol A epoxy resin, and continuing stirring for 10min to prepare infrared shielding treatment liquid;
(4) Immersing 75D/36F polyester fibers in an ethylenediamine water solution with the mass fraction of 0.8-1%, standing at 70 ℃ for 30min, taking out, washing with absolute ethyl alcohol for 5 times, and drying at 70 ℃ for 4 hours to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 8min at 30 ℃ and 35kHz, taking out until no drop exists for 40s, sequentially standing for 4min at 120 ℃, standing for 1h at 70 ℃, and standing for 12h at 50 ℃ and 100Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into a fiber with gram weight of 200g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
Comparative example 1
The preparation method of the fabric with the infrared shielding function mainly comprises the following preparation steps:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to a mass ratio of 1:130, stirring at 25 ℃ for reaction for 35min at 250r/min, adding cesium hydroxide monohydrate with the molar weight of tungsten chloride being 0.32 times, continuously stirring for 25min, adding absolute acetic acid with the mass of tungsten chloride being 35 times, continuously stirring for 17min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 215 ℃ for 22h, cooling to room temperature, centrifugally separating, and drying at 12.5 ℃ for 7h at 30Pa to obtain nano cesium tungsten bronze; uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.15% according to the mass ratio of 5:3.5:2:1, stirring and refluxing at 67.5 ℃ for 25min at 250r/min, adding nano cesium tungsten bronze with the mass of 0.8-1 times of that of the allyl trimethoxysilane, continuously stirring and refluxing for 70min, adding a hydrochloric acid aqueous solution with the mass fraction of 0.15% and the mass fraction of 0.25 times of that of the 3-glycidoxy propyl dimethoxy silane and the allyl trimethoxysilane, continuously stirring and refluxing for 45min, centrifugally separating and washing for 4 times by using absolute ethyl alcohol to obtain modified nano cesium tungsten bronze;
(2) Uniformly mixing heptafluorobutyric acid, thionyl chloride and tetrahydrofuran according to the mass ratio of 1:5.5:0.035, stirring and reacting for 55min at 45 ℃ and 400r/min, heating to 65 ℃ and stirring and refluxing for 2.5h, and drying for 5h at 95 ℃ to obtain heptafluorobutyryl chloride; uniformly mixing heptafluorobutyryl chloride and allylamine according to a molar ratio of 1:2.5, adding triethylamine with the mass of 0.35 times that of the heptafluorobutyryl chloride, stirring at 2.5 ℃ and 400r/min for 2.5 hours, and drying at 95 ℃ for 5 hours to obtain N-allyl heptafluorobutyramide; weighing according to the molar ratio of silicon-hydrogen bond in 202 methyl hydrogen-containing silicone oil, the molar ratio of the middle vinyl of 1, 7-divinyl-octamethyl tetrasiloxane and the allyl in N-allyl heptafluoro-butyramide of 1:0.5:0.15, uniformly mixing 202 methyl hydrogen-containing silicone oil, 1, 7-divinyl-octamethyl tetrasiloxane and N-allyl heptafluoro-butyramide, and adding chloroplatinic acid with the mass of 0.004 times that of 202 methyl hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing bisphenol A epoxy resin, modified nano cesium tungsten bronze, mixed silicon liquid and paraxylene according to the mass ratio of 7:3.3:4.5:1, stirring at 25 ℃ for 22.5min at 250r/min, adding poly N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.27 times that of bisphenol A epoxy resin, and continuously stirring for 9min to prepare infrared shielding treatment liquid;
(4) Immersing 75D/36F polyester fibers in an ethylenediamine water solution with the mass fraction of 0.9%, standing at 60 ℃ for 25min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 5h to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 7min at 25 ℃ and 30kHz, taking out until 35s are free from dripping, sequentially standing for 4.5min at 115 ℃, standing for 1.5h at 65 ℃ and standing for 11h at 45 ℃ and 75Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into a fiber with gram weight of 200g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
Comparative example 2
The preparation method of the fabric with the infrared shielding function mainly comprises the following preparation steps:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to a mass ratio of 1:130, adding chromium trichloride hexahydrate with a molar quantity of 0.15 times of the tungsten chloride, stirring at 25 ℃ for reaction for 35min at 250r/min, adding cesium hydroxide monohydrate with a molar quantity of 0.32 times of the tungsten chloride, continuously stirring for 25min, adding absolute acetic acid with a mass of 35 times of the tungsten chloride, continuously stirring for 17min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 215 ℃ for 22h, cooling to room temperature, centrifuging, separating, and drying at 12.5 ℃ for 7h at 30Pa to obtain chromium-doped nano cesium tungsten bronze;
(2) Uniformly mixing heptafluorobutyric acid, thionyl chloride and tetrahydrofuran according to the mass ratio of 1:5.5:0.035, stirring and reacting for 55min at 45 ℃ and 400r/min, heating to 65 ℃ and stirring and refluxing for 2.5h, and drying for 5h at 95 ℃ to obtain heptafluorobutyryl chloride; uniformly mixing heptafluorobutyryl chloride and allylamine according to a molar ratio of 1:2.5, adding triethylamine with the mass of 0.35 times that of the heptafluorobutyryl chloride, stirring at 2.5 ℃ and 400r/min for 2.5 hours, and drying at 95 ℃ for 5 hours to obtain N-allyl heptafluorobutyramide; weighing according to the molar ratio of silicon-hydrogen bond in 202 methyl hydrogen-containing silicone oil, the molar ratio of the middle vinyl of 1, 7-divinyl-octamethyl tetrasiloxane and the allyl in N-allyl heptafluoro-butyramide of 1:0.5:0.15, uniformly mixing 202 methyl hydrogen-containing silicone oil, 1, 7-divinyl-octamethyl tetrasiloxane and N-allyl heptafluoro-butyramide, and adding chloroplatinic acid with the mass of 0.004 times that of 202 methyl hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing bisphenol A epoxy resin, chromium-doped nano cesium tungsten bronze, mixed silicon liquid and paraxylene according to the mass ratio of 7:3.3:4.5:1, stirring at 25 ℃ for 22.5min at 250r/min, adding poly N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.27 times that of bisphenol A epoxy resin, and continuously stirring for 9min to prepare infrared shielding treatment liquid;
(4) Immersing 75D/36F polyester fibers in an ethylenediamine water solution with the mass fraction of 0.9%, standing at 60 ℃ for 25min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 5h to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 7min at 25 ℃ and 30kHz, taking out until 35s are free from dripping, sequentially standing for 4.5min at 115 ℃, standing for 1.5h at 65 ℃ and standing for 11h at 45 ℃ and 75Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into a fiber with gram weight of 200g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
Comparative example 3
The preparation method of the fabric with the infrared shielding function mainly comprises the following preparation steps:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to a mass ratio of 1:130, adding chromium trichloride hexahydrate with a molar quantity of 0.15 times of the tungsten chloride, stirring at 25 ℃ for reaction for 35min at 250r/min, adding cesium hydroxide monohydrate with a molar quantity of 0.32 times of the tungsten chloride, continuously stirring for 25min, adding absolute acetic acid with a mass of 35 times of the tungsten chloride, continuously stirring for 17min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 215 ℃ for 22h, cooling to room temperature, centrifuging, separating, and drying at 12.5 ℃ for 7h at 30Pa to obtain chromium-doped nano cesium tungsten bronze; uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.15% according to the mass ratio of 5:3.5:2:1, stirring and refluxing at 67.5 ℃ for 25min at 250r/min, adding chromium-doped nano cesium tungsten bronze with the mass of 0.8-1 times of the allyl trimethoxysilane, continuously stirring and refluxing for 70min, adding a hydrochloric acid aqueous solution with the mass fraction of 0.15% and the mass fraction of 0.25 times of the 3-glycidoxy propyl dimethoxy silane and the allyl trimethoxysilane, continuously stirring and refluxing for 45min, centrifugally separating and washing for 4 times by using absolute ethyl alcohol to obtain modified chromium-doped nano cesium tungsten bronze;
(2) Weighing according to the molar ratio of silicon-hydrogen bond in 202 methyl hydrogen-containing silicone oil to the molar ratio of the vinyl in 1, 7-divinyl-octamethyl tetrasiloxane of 1:0.65, uniformly mixing the 202 methyl hydrogen-containing silicone oil and the 1, 7-divinyl-octamethyl tetrasiloxane, adding chloroplatinic acid with the mass of 0.004 times that of the 202 methyl hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing bisphenol A epoxy resin, modified chromium doped nano cesium tungsten bronze, mixed silicon liquid and paraxylene according to the mass ratio of 7:3.3:4.5:1, stirring at 25 ℃ for 22.5min at 250r/min, adding poly N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.27 times that of bisphenol A epoxy resin, and continuously stirring for 9min to prepare infrared shielding treatment liquid;
(4) Immersing 75D/36F polyester fibers in an ethylenediamine water solution with the mass fraction of 0.9%, standing at 60 ℃ for 25min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 5h to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 7min at 25 ℃ and 30kHz, taking out until 35s are free from dripping, sequentially standing for 4.5min at 115 ℃, standing for 1.5h at 65 ℃ and standing for 11h at 45 ℃ and 75Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into a fiber with gram weight of 200g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
Comparative example 4
The preparation method of the fabric with the infrared shielding function mainly comprises the following preparation steps:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to a mass ratio of 1:130, adding chromium trichloride hexahydrate with a molar quantity of 0.15 times of the tungsten chloride, stirring at 25 ℃ for reaction for 35min at 250r/min, adding cesium hydroxide monohydrate with a molar quantity of 0.32 times of the tungsten chloride, continuously stirring for 25min, adding absolute acetic acid with a mass of 35 times of the tungsten chloride, continuously stirring for 17min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at 215 ℃ for 22h, cooling to room temperature, centrifuging, separating, and drying at 12.5 ℃ for 7h at 30Pa to obtain chromium-doped nano cesium tungsten bronze; uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.15% according to the mass ratio of 5:3.5:2:1, stirring and refluxing at 67.5 ℃ for 25min at 250r/min, adding chromium-doped nano cesium tungsten bronze with the mass of 0.8-1 times of the allyl trimethoxysilane, continuously stirring and refluxing for 70min, adding a hydrochloric acid aqueous solution with the mass fraction of 0.15% and the mass fraction of 0.25 times of the 3-glycidoxy propyl dimethoxy silane and the allyl trimethoxysilane, continuously stirring and refluxing for 45min, centrifugally separating and washing for 4 times by using absolute ethyl alcohol to obtain modified chromium-doped nano cesium tungsten bronze;
(2) Uniformly mixing bisphenol A epoxy resin, modified chromium doped nano cesium tungsten bronze and paraxylene according to a mass ratio of 7:3.3:1, stirring at 25 ℃ for 22.5min at 250r/min, adding poly N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.27 times that of the bisphenol A epoxy resin, and continuously stirring for 9min to prepare infrared shielding treatment liquid;
(3) Immersing 75D/36F polyester fibers in an ethylenediamine water solution with the mass fraction of 0.9%, standing at 60 ℃ for 25min, taking out, washing with absolute ethyl alcohol for 4 times, and drying at 65 ℃ for 5h to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 7min at 25 ℃ and 30kHz, taking out until 35s are free from dripping, sequentially standing for 4.5min at 115 ℃, standing for 1.5h at 65 ℃ and standing for 11h at 45 ℃ and 75Pa to obtain the infrared shielding fiber; the infrared shielding fiber is woven into a fiber with gram weight of 200g/m by a weaving machine 2 The fabric with the infrared shielding function is the fabric.
Test example 1
Testing of infrared shielding properties
Preparation of the sample: the infrared shielding treatment solutions of examples 1 to 3 and comparative examples 1 to 4 were applied to glass sheets, and were sequentially left to stand at 115℃for 4.5 minutes, at 65℃for 1.5 hours, and at 45℃for 11 hours at 75Pa, to prepare film-like samples having a thickness of 10. Mu.m.
The testing method adopts a Lambda750 type ultraviolet-visible near infrared spectrophotometer to measure, the scanning speed is 240nm/min, the slit width is 2.0nm, and the near infrared transmittance with the wavelength of 780-2500 nm is measured and recorded. The results are shown in Table 1
TABLE 1
Near infrared transmittance Near infrared transmittance
Example 1 7.92％ Comparative example 1 16.85％
Example 2 8.13％ Comparative example 2 14.47％
Example 3 8.26％ Comparative example 3 8.08％
Comparative example 4 8.14％
From comparison of experimental data of examples 1 to 3 and comparative examples 1 to 4 in table 1, it can be found that the fabric with infrared shielding function prepared by the invention has good infrared shielding performance.
From comparison of experimental data of examples 1, 2 and 3 and comparative example 1, it can be found that the near infrared transmittance of examples 1, 2 and 3 compared with comparative example 1 is low, which indicates that chromium doping is performed on nano cesium tungsten bronze, and as chromium and tungsten belong to the same subgroup and the ion radius is close, the doping can partially replace tungsten, so that crystal defects are further increased, and the infrared shielding performance is improved; from comparison of experimental data of examples 1, 2 and 3 and comparative example 2, the near infrared transmittance of examples 1, 2 and 3 compared with comparative example 2 is low, which indicates that the modified chromium-doped nano cesium tungsten bronze is modified to form polysiloxane long chains on the surface of the modified chromium-doped nano cesium tungsten bronze, so that the compatibility of the chromium-doped nano cesium tungsten bronze with other components is improved, the chromium-doped nano cesium tungsten bronze is not easy to agglomerate, and the infrared shielding performance is improved.
Test example 2
Testing of fracture resistance and acid-base resistance
Preparation of the sample: the infrared shielding fibers of examples 1 to 3 and comparative examples 1 to 4 were sampled to a length of 1m, and their mass was weighed on an electronic balance to calculate the line density.
The anti-fracture performance test method comprises the following steps: and (5) taking a 50mm sample wire, clamping the sample wire in an upper clamp holder and a lower clamp holder of a strength tester for stretching until the sample wire breaks, and calculating breaking strength.
The acid and alkali resistance testing method comprises the following steps: sample wires of 50mm are taken, soaked in 5% hydrochloric acid and 5% sodium hydroxide solution for 30 days, respectively, taken out, washed with pure water for 3 times, dried, and the breaking strength is measured again, and the change rate=1-breaking strength after acid-alkali leaching/initial breaking strength is calculated. The results are shown in Table 2.
TABLE 2
From comparison of experimental data of examples 1 to 3 and comparative examples 1 to 4 in table 2, it can be found that the fabric with infrared shielding function prepared by the invention has good fracture resistance and acid and alkali resistance.
As can be found from the comparison of experimental data of examples 1, 2 and 3 and comparative example 2, the examples 1, 2 and 3 have high breaking strength and low change rate compared with comparative example 2, which indicates that the modified chromium-doped nano cesium tungsten bronze has a polysiloxane long chain formed on the surface, so that the dispersibility of the chromium-doped nano cesium tungsten bronze is improved, meanwhile, the polysiloxane long chain contains a large number of carbon-carbon double bonds and epoxy groups, the carbon-carbon double bonds can react with silicon hydrogen bonds on hydrogen-containing silicone oil in a hydrosilylation manner, and the epoxy groups can react with amino groups, so that a crosslinked network structure is formed, the structure is more compact and stable, and the fracture resistance and acid-alkali resistance are improved; from comparison of experimental data of examples 1, 2 and 3 and comparative example 3, the low change rate of examples 1, 2 and 3 compared with comparative example 3 shows that the addition of N-allyl heptafluorobutyramide introduces a heptafluorobutyramide branched chain on hydrogen-containing silicone oil, has good protection effect on a main chain, effectively relieves the erosion of corrosive medium, and improves acid and alkali resistance; from comparison of experimental data of examples 1, 2 and 3 and comparative example 4, it can be found that the examples 1, 2 and 3 and comparative example 4 have high breaking strength and low change rate, which indicates that the addition of the mixed silicon liquid, which is subjected to hydrosilylation reaction, and crosslinked and cured with epoxy resin, interpenetrates to form an interpenetrating network structure, thereby improving fracture resistance and acid-base resistance.
The thermal insulation antistatic silk fiber materials obtained in each example and the comparative example are taken to obtain sample silk with the length of 1m, the mass of the sample silk is weighed on an electronic balance, the line density is calculated, and the sample silk with the length of 50mm is taken and clamped in an upper clamp holder and a lower clamp holder of a strength meter. And (5) stretching according to the set linear density and the set stretching speed until the sample wire breaks. The breaking strength is automatically printed out by the electronic single yarn strength tester. The results are shown in Table 2.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (5)

1. The preparation method of the fabric with the infrared shielding function is characterized by comprising the following preparation steps of:
(1) Uniformly mixing tungsten chloride and absolute ethyl alcohol according to the mass ratio of 1:120-140, adding hexahydrated chromium trichloride with the molar quantity of tungsten chloride of 0.14-0.16 times, stirring at the temperature of 20-30 ℃ for reaction for 30-40 min at the speed of 200-300 r/min, adding cesium hydroxide monohydrate with the molar quantity of tungsten chloride of 0.3-0.34 times, continuously stirring for 20-30 min, adding absolute acetic acid with the mass of 30-40 times of tungsten chloride, continuously stirring for 10-15 min, transferring into a high-pressure reaction kettle, sealing the high-pressure reaction kettle, reacting at the temperature of 210-220 ℃ for 20-24 h, cooling to room temperature, centrifugally separating, drying at the temperature of 10-15 ℃ for 6-8 h at the speed of 10-50 Pa, and obtaining chromium-doped nano cesium tungsten bronze; uniformly mixing allyl trimethoxysilane, dimethyl dimethoxy silane, methanol and a hydrochloric acid aqueous solution with the mass fraction of 0.1-0.2% according to the mass ratio of 4-6:3-4:2:1, stirring and refluxing for 20-30 min at 65-70 ℃ and 200-300 r/min, adding chromium doped nano cesium tungsten bronze with the mass of 0.8-1 times of the allyl trimethoxysilane, continuously stirring and refluxing for 60-80 min, adding 3-glycidoxypropyl dimethoxy silane with the mass of 0.2-0.3 times of the allyl trimethoxysilane and a hydrochloric acid aqueous solution with the mass fraction of 0.1-0.2% with the mass fraction of 0.04-0.06 times of the allyl trimethoxysilane, continuously stirring and refluxing for 40-50 min, centrifugally separating and washing 3-5 times with absolute ethyl alcohol to obtain modified chromium doped nano cesium tungsten bronze;
(2) Uniformly mixing heptafluorobutyric acid, thionyl chloride and tetrahydrofuran according to the mass ratio of 1:5-6:0.03-0.04, stirring at the temperature of 40-50 ℃ for reaction for 50-60 min at the speed of 300-500 r/min, heating to the temperature of 60-70 ℃, stirring and refluxing for 2-3 h, and drying at the temperature of 90-100 ℃ for 4-6 h to obtain heptafluorobutyryl chloride; uniformly mixing heptafluorobutyryl chloride and allylamine according to a molar ratio of 1:2-3, adding triethylamine with the mass of 0.3-0.4 times that of the heptafluorobutyryl chloride, stirring for 2-3 hours at the temperature of 0-5 ℃ and the speed of 300-500 r/min, and drying for 4-6 hours at the temperature of 90-100 ℃ to prepare N-allyl heptafluorobutyramide; weighing according to the molar ratio of silicon-hydrogen bond in hydrogen-containing silicone oil to vinyl in 1, 7-divinyl-octamethyltetrasiloxane to allyl in N-allyl heptafluorobutyramide of 1:0.4-0.6:0.1-0.2, uniformly mixing the hydrogen-containing silicone oil, the 1, 7-divinyl-octamethyltetrasiloxane and the N-allyl heptafluorobutyramide, and adding chloroplatinic acid with the mass of 0.003-0.005 times that of the hydrogen-containing silicone oil, and uniformly mixing to prepare mixed silicon liquid;
(3) Uniformly mixing epoxy resin, modified chromium-doped nano cesium tungsten bronze, mixed silicon liquid and dimethylbenzene according to a mass ratio of 6-8:3-3.5:4-5:1, stirring for 20-25 min at 20-30 ℃ at 200-300 r/min, adding poly-N-aminoethyl-3-aminopropyl methyl siloxane with the mass of 0.25-0.3 times of that of the epoxy resin, and continuously stirring for 8-10 min to prepare an infrared shielding treatment liquid;
(4) Immersing polyester fibers in an ethylenediamine water solution with the mass fraction of 0.8-1%, standing for 20-30 min at 50-70 ℃, taking out, washing with absolute ethyl alcohol for 3-5 times, and drying for 4-6 h at 60-70 ℃ to obtain aminolysis polyester fibers; immersing the aminolysis polyester fiber in an infrared shielding treatment liquid, carrying out ultrasonic treatment for 6-8 min at 20-30 ℃ and 25-35 kHz, taking out until 30-40 s have no dripping, sequentially standing for 4-5 min at 110-120 ℃, standing for 1-2 h at 60-70 ℃, and standing for 10-12 h at 40-50 ℃ and 50-100 Pa to obtain the infrared shielding fiber; passing infrared shielding fibers throughWeaving with a weaving machine to obtain a woven fabric with gram weight of 200-300 g/m 2 The fabric with the infrared shielding function is the fabric.
2. The method for preparing the fabric with the infrared shielding function according to claim 1, wherein the hydrogen-containing silicone oil in the step (2) is 202 methyl hydrogen-containing silicone oil.
3. The method for preparing the fabric with the infrared shielding function according to claim 1, wherein the epoxy resin in the step (3) is bisphenol A type epoxy resin; the dimethylbenzene is one or more of paraxylene, metaxylene and orthoxylene.
4. The method for preparing the fabric with the infrared shielding function according to claim 1, wherein the polyester fibers in the step (4) are 75D/36F polyester fibers.
5. A fabric with an infrared shielding function prepared by the method for preparing a fabric with an infrared shielding function according to any one of claims 1 to 4.
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